CN104773730A - Method for preparing graphene - Google Patents
Method for preparing graphene Download PDFInfo
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- CN104773730A CN104773730A CN201510211761.6A CN201510211761A CN104773730A CN 104773730 A CN104773730 A CN 104773730A CN 201510211761 A CN201510211761 A CN 201510211761A CN 104773730 A CN104773730 A CN 104773730A
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Abstract
The invention discloses a method for preparing graphene. The method comprises the following steps that a graghite rod is soaked in inorganic salt solution until the graghite rod is soaked fully; the fully-soaked graghite rid serves as a positive pole, a metal electrode serves as a negative pole, the inorganic salt solution serves as electrolyte solution, a electrolytic cell is assembled, and a constant voltage is imposed between the negative pole and the positive pole to conduct electrochemical stripping; the positive pole and the negative pole are taken out after electrochemical stripping is finished, the electrolyte solution is retained, and ultrasonic treatment is conducted on the electrolyte solution; supernatant liquid is retained after the electrolyte solution after being conducted the ultrasonic treatment is centrifuged, the supernatant liquid is aquoeous solution of graphene, residue is retained after the supernatant liquid of the graphene is filtered, washing and drying are conducted on the residue, and the graphene is obtained. According to the method for preparing the graphene, the thin-layer graphene is produced through electrochemical intercalation and expansive action, and the produced graphene lamella is comparatively thin.
Description
Technical field
The present invention relates to Materials Science and Engineering field, particularly relate to a kind of preparation method of Graphene.
Background technology
Graphene (graphene) is that what to be made up of carbon atom take six-ring as the monoatomic layer material of elementary cell.Graphene both can have been piled up becomes 3D graphite, also curlingly can become 1D carbon nanotube, even can be rolled into 0D soccerballene.On two dimensional surface, sp
2the carbon atom of hydridization is connected with adjacent three carbon atoms by strong σ key, and remaining P electronic orbit, perpendicular to graphene planes, forms large π key with the atom of surrounding, makes Graphene have good electroconductibility.Graphene not only to have contained the abundant and physical phenomenon of novelty, there is important theoretical investigation be worth, and the structure of its uniqueness and excellent performance likely make it obtain great practical application in multiple field, for the economy in future, social development provide new strong growth point.The theoretical specific surface area of Graphene can reach 2630m
2g
-1.The intensity of Graphene can reach 130GPa, is more than 100 times of steel.The thermal conductivity of Graphene is adamantine 3 times, is approximately 5 × 103Wm
-1k
-1.The carrier mobility of Graphene is up to 2.5 × 105cm
2v
-1s
-1, be 100 times of business silicon chip mobility.These excellent specific properties of Graphene make it have huge potential application foreground in the field such as opto-electronic device, chemical power source (as solar cell, lithium ion battery), gas sensor, catalyzer and pharmaceutical carrier, antistatic and heat sink material.Therefore, carry out extensive and deep research to the related science technical problem in Graphene preparation, explore its application in above-mentioned field, having great scientific meaning and wide using value, is also one of study hotspot of current Graphene research field.
At present, the preparation method of Graphene mainly contains mechanically peel method, epitaxial crystal growth, chemical Vapor deposition process, graphite oxide reduction method etc.Wherein, mechanically peel method can prepare the Graphene of micron size, but its controllability is lower, is difficult to realize extensive synthesis; The epitaxially grown Graphene of SiC, although directly make electron device by photoetching process, but because surface in high-temperature heating process, SiC crystal surface easily reconstructs, cause surface tissue comparatively complicated, be difficult to obtain the homogeneous Graphene of big area, thickness; Chemical Vapor deposition process is considered to prepare the good method of large-area graphene, but present stage technique immature and higher cost limit it and apply on a large scale; Graphite oxide reduction method normally obtains graphite oxide with the vitriol oil, SODIUMNITRATE and potassium permanganate oxidation flake graphite, then carrys out redox graphene by the method for high temperature pyrolysis after obtaining graphene oxide with ultrasonic stripping.Though chemical stripping method can prepare Graphene in a large number, but its violent redox processes can destroy the carbon skeleton of graphene planes, produce defect, the complicated technique of very high output and quality problems cause the Graphene Quality Down of gained, although can be had seriously to govern applying of Graphene.And electrochemical production Graphene has caused sufficient concern in recent years, the method without the need to using the strong oxidizers such as potassium permanganate, can avoid strong oxidizer to the destruction of graphene-structured and performance in preparation process; Without the need to using the inflammable and explosive substances hazardous materials such as basic metal (K, Na), do not introduce hazardous and noxious substances, environmental friendliness; Preparation condition is controlled; Cost is low, is applicable to scale operation.
But graphene sheet layer prepared by traditional electrochemical method is thicker, is not well positioned to meet the demand of practical application.
Summary of the invention
Based on this, be necessary to provide a kind of preparation method that can prepare the Graphene of the thinner Graphene of lamella.
A preparation method for Graphene, comprises the steps:
Graphite rod is immersed in inorganic salt solution until described graphite rod is fully infiltrated;
With the described graphite rod fully infiltrated for anode, take metal electrode as negative electrode, using described inorganic salt solution as electrolytic solution, be assembled into electrolyzer system, between described negative electrode and described anode, apply constant voltage carry out electrochemical stripping;
After electrochemical stripping completes, take out described anode and described negative electrode, retain described electrolytic solution and supersound process is carried out to described electrolytic solution; And
The centrifugal rear reservation supernatant liquid of described electrolytic solution supersound process crossed, described supernatant liquid is the aqueous solution of Graphene, retains filter residue after being filtered by the aqueous solution of described Graphene, washs and drying, obtain Graphene to described filter residue.
In one embodiment, the specpure graphite of the material of described graphite rod to be granular size be 0.01mm ~ 5mm.
In one embodiment, described inorganic salt solution is selected from the one in sodium stannate solution and potassium stannate solution.
In one embodiment, the concentration of described inorganic salt solution is 0.1mol/L ~ 1mol/L.
In one embodiment, to be immersed in by graphite rod in described inorganic salt solution until described graphite rod is by the operation that fully infiltrates, the described graphite rod time be immersed in described inorganic salt solution is 1h ~ 2h.
In one embodiment, the material of described metal electrode is selected from the one in platinum, gold and silver, copper, titanium and nickel.
In one embodiment, apply constant voltage and carry out in the operation of electrochemical stripping between described negative electrode and described anode, the scope of described constant voltage is 1V ~ 10V.
In one embodiment, apply constant voltage and carry out in the operation of electrochemical stripping between described negative electrode and described anode, the time of described electrochemical stripping is 30min ~ 240min.
In one embodiment, carry out in the operation of supersound process to described electrolytic solution, the time of described supersound process is 30min ~ 120min.
In one embodiment, in the operation that described electrolytic solution supersound process crossed is centrifugal, described centrifugal rotating speed is 1000rpm ~ 5000rpm, and the described centrifugal time is 30min ~ 60min.
The preparation method of this Graphene first obtains the electrolytic solution containing Graphene by electrochemical stripping graphite rod, then by electrolytic solution supersound process, finally centrifugal to electrolytic solution, and the supernatant liquid of reservation filters, washing, obtain Graphene after drying.The preparation method of this Graphene obtains thin graphene by electrochemical intercalation and expansion, and relative to graphene sheet layer prepared by traditional electrochemical method, the graphene sheet layer that the preparation method of this Graphene obtains is thinner.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the Graphene of an embodiment;
Fig. 2 is the TEM photo of the Graphene that embodiment 1 obtains;
Fig. 3 is the Raman figure of the Graphene that embodiment 1 obtains.
Embodiment
Mainly in conjunction with the drawings and the specific embodiments the preparation method of Graphene is described in further detail below.
The preparation method of the Graphene of an embodiment as shown in Figure 1, comprises the steps:
S10, graphite rod to be immersed in inorganic salt solution until graphite rod is fully infiltrated.
The material of graphite rod can be the specpure graphite of 0.01mm ~ 5mm for granular size.Can pre-treatment be carried out to graphite rod, namely adopt sand paper by the scrubbing of graphite rod surface finish.
Inorganic salt solution is selected from sodium stannate (Na
2snO
3) solution and potassium stannate (K
2snO
3) one in solution.Negatively charged ion stannate radicle ion (SnO contained in sodium stannate and potassium stannate
3 2-) size and graphite flake layer between distance (0.34nm) suitable, can intercalation enter graphite lamella between so that the model ylid bloom action power that reduces between graphite flake layer, be conducive to stripping and obtain thin graphene.
The concentration of inorganic salt solution can be 0.1mol/L ~ 1mol/L.
In S10, the graphite rod time be immersed in inorganic salt solution is 1h ~ 2h.
S20, the graphite rod of abundant infiltration that obtains with S10, for anode, take metal electrode as negative electrode, using above-mentioned inorganic salt solution as electrolytic solution, are assembled into electrolyzer system, apply constant voltage and carry out electrochemical stripping between negative electrode and positive electrode.
The material of metal electrode is selected from the one in platinum, gold and silver, copper, titanium and nickel.
In S20, the scope of constant voltage is 1V ~ 10V, and the time of electrochemical stripping is 30min ~ 240min.
S30, after electrochemical stripping completes, take out anode and negative electrode, retain electrolytic solution and supersound process is carried out to electrolytic solution.
In S30, the time of supersound process is 30min ~ 120min, to improve Graphene dispersiveness in aqueous further.
The centrifugal rear reservation supernatant liquid of electrolytic solution that S40, the supersound process obtained by S30 are crossed, supernatant liquid is the aqueous solution of Graphene, retains filter residue after being filtered by the aqueous solution of Graphene, washs and drying, obtain Graphene to filter residue.
In S40, centrifugal rotating speed is 1000pm ~ 5000rpm, and the centrifugal time is 30min ~ 60min.
In the operation of filter the aqueous solution of Graphene, filter the method that can adopt suction filtration.
The preparation method of this Graphene first obtains the electrolytic solution containing Graphene by electrochemical stripping graphite rod, then by electrolytic solution supersound process, finally centrifugal to electrolytic solution, and the supernatant liquid of reservation filters, washing, obtain Graphene after drying.The preparation method of this Graphene is by ion insertion graphite flake layer, thus the Van der Waals force between reduction graphite flake layer, and then reach top layer graphite and to come off obtained thin graphene, relative to graphene sheet layer prepared by traditional electrochemical method, the graphene sheet layer that the preparation method of this Graphene obtains is thinner.
The preparation method of this Graphene, without the need to using the strong oxidizers such as potassium permanganate, can avoid strong oxidizer to the destruction of graphene-structured and performance; Without the need to using the inflammable and explosive substances hazardous materials such as basic metal, oleum, hydrogen peroxide, not using the poisonous reductive agents such as hydrazine hydrate yet, not introducing hazardous and noxious substances, production safety, environmental friendliness.
In addition, the number of plies of the Graphene that the preparation method of this Graphene obtains is 1 ~ 50 layer, and lamella is thinner, and obtained Graphene defect is few, and quality is high.
Meanwhile, preparation method's flow process of this Graphene is simple, easy handling, and cost is low, and productive rate is high, and reaction conditions is gentle, and energy consumption is low, is applicable to industrialization scale operation.
Be specific embodiment below.
Embodiment 1
Get graphite rod, stand-by by giving over to after its surface finish scrubbing with sand paper.Preparation 100mL concentration is the Na of 0.1mol/L
2snO
3solution, is immersed in Na by graphite rod
2snO
3after solution 1h makes graphite rod fully be infiltrated, with the graphite rod fully infiltrated for anode, be negative electrode with platinum plate electrode, with Na
2snO
3solution is electrolytic solution, is assembled into electrolyzer system.Apply the operating voltage of 10V between a cathode and an anode, after continuing electrochemical stripping 120min, powered-down stops peeling off.Carry out supersound process 1h to electrolytic solution after taking out negative electrode and anode, then centrifugal 20min under 3000rmp/min, the supernatant liquid of reservation is the aqueous solution of Graphene.The aqueous solution of Graphene is carried out suction filtration, washing, drying successively, obtains graphene powder.
The aqueous solution of the Graphene obtained by embodiment 1 carries out tem observation, obtains Fig. 2, and the graphene powder obtained by embodiment 1 carries out Raman sign, obtains Fig. 3.
As seen from Figure 2, the lamella of the Graphene that embodiment 1 is obtained is thinner.
As seen from Figure 3, the I of the Graphene that embodiment 1 is obtained
d/ I
g(~ 1.3) are less, illustrate that the obtained less quality of Graphene defect is higher.
Embodiment 2
Get graphite rod, stand-by by giving over to after its surface finish scrubbing with sand paper.Preparation 100mL concentration is the Na of 0.2mol/L
2snO
3solution, is immersed in Na by graphite rod
2snO
3after solution 2h makes graphite rod fully be infiltrated, with the graphite rod fully infiltrated for anode, be negative electrode with platinum plate electrode, with Na
2snO
3solution is electrolytic solution, is assembled into electrolyzer system.Apply the operating voltage of 10V between a cathode and an anode, after continuing electrochemical stripping 30min, powered-down stops peeling off.Carry out supersound process 1h to electrolytic solution after taking out negative electrode and anode, then centrifugal 20min under 3000rmp/min, the supernatant liquid of reservation is the aqueous solution of Graphene.The aqueous solution of Graphene is carried out suction filtration, washing, drying successively, obtains graphene powder.
Embodiment 3
Get graphite rod, stand-by by giving over to after its surface finish scrubbing with sand paper.Preparation 100mL concentration is the Na of 0.4mol/L
2snO
3solution, is immersed in Na by graphite rod
2snO
3after solution 1.5h makes graphite rod fully be infiltrated, with the graphite rod fully infiltrated for anode, be negative electrode with platinum plate electrode, with Na
2snO
3solution is electrolytic solution, is assembled into electrolyzer system.Apply the operating voltage of 6V between a cathode and an anode, after continuing electrochemical stripping 150min, powered-down stops peeling off.Carry out supersound process 2h to electrolytic solution after taking out negative electrode and anode, then centrifugal 20min under 3000rmp/min, the supernatant liquid of reservation is the aqueous solution of Graphene.The aqueous solution of Graphene is carried out suction filtration, washing, drying successively, obtains graphene powder.
Embodiment 4
Get graphite rod, stand-by by giving over to after its surface finish scrubbing with sand paper.Preparation 100mL concentration is the Na of 0.6mol/L
2snO
3solution, is immersed in Na by graphite rod
2snO
3after solution 1h makes graphite rod fully be infiltrated, with the graphite rod fully infiltrated for anode, with titanium sheet electrode for negative electrode, with Na
2snO
3solution is electrolytic solution, is assembled into electrolyzer system.Apply the operating voltage of 4V between a cathode and an anode, after continuing electrochemical stripping 240min, powered-down stops peeling off.Carry out supersound process 1h to electrolytic solution after taking out negative electrode and anode, then centrifugal 20min under 3000rmp/min, the supernatant liquid of reservation is the aqueous solution of Graphene.The aqueous solution of Graphene is carried out suction filtration, washing, drying successively, obtains graphene powder.
Embodiment 5
Get graphite rod, stand-by by giving over to after its surface finish scrubbing with sand paper.The K of preparation 100mL concentration 0.8mol/L
2snO
3solution, is immersed in K by graphite rod
2snO
3after solution 1h makes graphite rod fully be infiltrated, with the graphite rod fully infiltrated for anode, with nickel sheet electrode for negative electrode, with K
2snO
3solution is electrolytic solution, is assembled into electrolyzer system.Apply the operating voltage of 10V between a cathode and an anode, after continuing electrochemical stripping 120min, powered-down stops peeling off.Carry out supersound process 1h to electrolytic solution after taking out negative electrode and anode, then centrifugal 20min under 3000rmp/min, the supernatant liquid of reservation is the aqueous solution of Graphene.The aqueous solution of Graphene is carried out suction filtration, washing, drying successively, obtains graphene powder.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. utilize a method for preparing graphene by electrochemical stripping, it is characterized in that, comprise the steps:
Graphite rod is immersed in inorganic salt solution until described graphite rod is fully infiltrated;
With the described graphite rod fully infiltrated for anode, take metal electrode as negative electrode, using described inorganic salt solution as electrolytic solution, be assembled into electrolyzer system, between described negative electrode and described anode, apply constant voltage carry out electrochemical stripping;
After electrochemical stripping completes, take out described anode and described negative electrode, retain described electrolytic solution and supersound process is carried out to described electrolytic solution; And
The centrifugal rear reservation supernatant liquid of described electrolytic solution supersound process crossed, described supernatant liquid is the aqueous solution of Graphene, retains filter residue after being filtered by the aqueous solution of described Graphene, washs and drying, obtain Graphene to described filter residue.
2. the preparation method of Graphene as claimed in claim 1, is characterized in that, the specpure graphite of the material of described graphite rod to be granular size be 0.01mm ~ 5mm.
3. the preparation method of Graphene as claimed in claim 1, it is characterized in that, described inorganic salt solution is selected from the one in sodium stannate solution and potassium stannate solution.
4. the preparation method of Graphene as claimed in claim 1, it is characterized in that, the concentration of described inorganic salt solution is 0.1mol/L ~ 1mol/L.
5. the preparation method of Graphene as claimed in claim 1, is characterized in that, to be immersed in by graphite rod in described inorganic salt solution until described graphite rod is by the operation that fully infiltrates, the described graphite rod time be immersed in described inorganic salt solution is 1h ~ 2h.
6. the preparation method of Graphene as claimed in claim 1, it is characterized in that, the material of described metal electrode is selected from the one in platinum, gold and silver, copper, titanium and nickel.
7. the preparation method of Graphene as claimed in claim 1, it is characterized in that, between described negative electrode and described anode, apply constant voltage carry out in the operation of electrochemical stripping, the scope of described constant voltage is 1V ~ 10V.
8. the preparation method of Graphene as claimed in claim 1, it is characterized in that, between described negative electrode and described anode, apply constant voltage carry out in the operation of electrochemical stripping, the time of described electrochemical stripping is 30min ~ 240min.
9. the preparation method of Graphene as claimed in claim 1, it is characterized in that, carry out in the operation of supersound process to described electrolytic solution, the time of described supersound process is 30min ~ 120min.
10. the preparation method of Graphene as claimed in claim 1, it is characterized in that, in the operation that described electrolytic solution supersound process crossed is centrifugal, described centrifugal rotating speed is 1000rpm ~ 5000rpm, and the described centrifugal time is 30min ~ 60min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347330A (en) * | 2015-11-06 | 2016-02-24 | 新乡远东电子科技有限公司 | Preparation method of high specific surface area graphene |
| CN105845903A (en) * | 2016-03-31 | 2016-08-10 | 中国科学院深圳先进技术研究院 | High-thermal-conductivity flexible graphene composite material and preparation method therefor, and lithium ion battery |
| CN105948025A (en) * | 2016-05-05 | 2016-09-21 | 德阳烯碳科技有限公司 | Method for electrochemically preparing graphene |
| CN107235487A (en) * | 2016-03-23 | 2017-10-10 | 上海新池能源科技有限公司 | The preparation method of graphene |
| CN108502874A (en) * | 2017-02-28 | 2018-09-07 | 上海华明高技术（集团）有限公司 | A kind of method that electrochemistry assisting ultrasonic method prepares graphene dispersing solution |
| PL422358A1 (en) * | 2017-07-26 | 2019-01-28 | Newave Technologies Spółka Z Ograniczoną Odpowiedzialnością | Method for synthesis of graphene and nano- and micro crystals of graphite |
| CN109328104A (en) * | 2016-06-26 | 2019-02-12 | 纳米技术仪器公司 | By coke or coal electrochemical production graphene film |
| CN109574355A (en) * | 2018-12-25 | 2019-04-05 | 浙江大学 | A kind of method of resource of the high containing sulfate Acid Dye Wastewater of high concentration |
| CN110357087A (en) * | 2019-08-14 | 2019-10-22 | 中国科学院兰州化学物理研究所 | A method of graphene oxide is prepared based on high concentration inorganic salt solution removing |
| CN110526235A (en) * | 2018-05-23 | 2019-12-03 | 浙江大学 | A method of oxygen doping three-dimensional grapheme in situ is prepared by electrochemical stripping |
| CN111017915A (en) * | 2018-10-10 | 2020-04-17 | 长春工业大学 | Method for preparing graphene from graphite |
| CN111732095A (en) * | 2020-07-16 | 2020-10-02 | 苏州碳素集电新材料有限公司 | Self-supporting graphene manganese dioxide nanowire composite film electrode and preparation method thereof |
| WO2020248462A1 (en) * | 2019-06-11 | 2020-12-17 | 中国科学院上海微系统与信息技术研究所 | Method for preparing high-quality graphene material |
| CN112481644A (en) * | 2020-11-10 | 2021-03-12 | 中国航发北京航空材料研究院 | Flower-shaped graphene, melt-blown fabric, preparation method of flower-shaped graphene and melt-blown fabric, and mask |
| CN113249741A (en) * | 2021-06-30 | 2021-08-13 | 桂林清研皓隆新材料有限公司 | Preparation method of graphene and graphene |
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| CN105347330B (en) * | 2015-11-06 | 2017-04-12 | 新乡市远东电子科技股份有限公司 | Preparation method of high specific surface area graphene |
| CN105347330A (en) * | 2015-11-06 | 2016-02-24 | 新乡远东电子科技有限公司 | Preparation method of high specific surface area graphene |
| CN107235487A (en) * | 2016-03-23 | 2017-10-10 | 上海新池能源科技有限公司 | The preparation method of graphene |
| CN107235487B (en) * | 2016-03-23 | 2019-09-06 | 上海新池能源科技有限公司 | The preparation method of graphene |
| CN105845903A (en) * | 2016-03-31 | 2016-08-10 | 中国科学院深圳先进技术研究院 | High-thermal-conductivity flexible graphene composite material and preparation method therefor, and lithium ion battery |
| CN105948025A (en) * | 2016-05-05 | 2016-09-21 | 德阳烯碳科技有限公司 | Method for electrochemically preparing graphene |
| CN109328104A (en) * | 2016-06-26 | 2019-02-12 | 纳米技术仪器公司 | By coke or coal electrochemical production graphene film |
| CN108502874A (en) * | 2017-02-28 | 2018-09-07 | 上海华明高技术（集团）有限公司 | A kind of method that electrochemistry assisting ultrasonic method prepares graphene dispersing solution |
| PL422358A1 (en) * | 2017-07-26 | 2019-01-28 | Newave Technologies Spółka Z Ograniczoną Odpowiedzialnością | Method for synthesis of graphene and nano- and micro crystals of graphite |
| CN110526235A (en) * | 2018-05-23 | 2019-12-03 | 浙江大学 | A method of oxygen doping three-dimensional grapheme in situ is prepared by electrochemical stripping |
| CN110526235B (en) * | 2018-05-23 | 2021-05-14 | 浙江大学 | Method for preparing in-situ oxygen-doped three-dimensional graphene through electrochemical stripping |
| CN111017915A (en) * | 2018-10-10 | 2020-04-17 | 长春工业大学 | Method for preparing graphene from graphite |
| CN109574355A (en) * | 2018-12-25 | 2019-04-05 | 浙江大学 | A kind of method of resource of the high containing sulfate Acid Dye Wastewater of high concentration |
| CN109574355B (en) * | 2018-12-25 | 2022-12-09 | 浙江大学 | Recycling method of high-concentration high-sulfur-content hydrochloric acid dye wastewater |
| WO2020248462A1 (en) * | 2019-06-11 | 2020-12-17 | 中国科学院上海微系统与信息技术研究所 | Method for preparing high-quality graphene material |
| CN110357087A (en) * | 2019-08-14 | 2019-10-22 | 中国科学院兰州化学物理研究所 | A method of graphene oxide is prepared based on high concentration inorganic salt solution removing |
| CN111732095A (en) * | 2020-07-16 | 2020-10-02 | 苏州碳素集电新材料有限公司 | Self-supporting graphene manganese dioxide nanowire composite film electrode and preparation method thereof |
| CN112481644A (en) * | 2020-11-10 | 2021-03-12 | 中国航发北京航空材料研究院 | Flower-shaped graphene, melt-blown fabric, preparation method of flower-shaped graphene and melt-blown fabric, and mask |
| CN113249741A (en) * | 2021-06-30 | 2021-08-13 | 桂林清研皓隆新材料有限公司 | Preparation method of graphene and graphene |
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